1、November 2009DEUTSCHE NORM English price group 11No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 67.200.20!$ZaG“155623
2、6www.din.deDDIN EN ISO 659Oilseeds Determination of oil content (Reference method) (ISO 659:2009)English version of DIN EN ISO 659:2009-11lsamen Bestimmung des lgehaltes (Referenzverfahren) (ISO 659:2009)Englische Fassung DIN EN ISO 659:2009-11SupersedesDIN EN ISO 659:1998-10www.beuth.deDocument com
3、prises 19 pagesDIN EN ISO 659:2009-11 2 National foreword This standard has been prepared by Technical Committee ISO/TC 34 “Food products” (Secretariat: AFNOR, France), Subcommittee SC 2 “Oleaginous seeds and fruits and oilseed meals” (Secretariat: AFNOR, France) in collaboration with Technical Comm
4、ittee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products Methods of sampling and analysis” (Secretariat: AFNOR, France). The responsible German bodies involved in its preparation were the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural
5、 Products Standards Committee) and the Deutsche Gesellschaft fr Fettwissenschaft e. V. (German Fat Research Society), Joint Committee Analytik von Fetten, len, Fettprodukten, verwandten Stoffen und Rohstoffen. The DIN Standards corresponding to the International Standards referred to in the EN are a
6、s follows: ISO 542 DIN EN ISO 542 ISO 658 DIN EN ISO 658 ISO 664 DIN EN ISO 664 ISO 665 DIN EN ISO 665 ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN EN ISO 659:1998-10 as follows: a) The scope now includes information regarding the “procedure for sunfl
7、ower seed”. b) In subclause 6.2, NOTE, the example of the ultra-centrifugal mill has been changed. c) In subclause 6.3, the examples of microgrinders have been changed. d) In subclause 6.5, information relating to the use of a Soxhlet siphoning-type extractor has been included. e) In subclause 6.7,
8、a warning note has been included. f) In subclause 8.3.4, sunflower seed and cottonseed have been excluded. g) A new subclause 8.3.5 “Sunflower seed” has been included. h) Clause 9 now includes general information regarding “single determinations”. i) The wording of clause 9 has been modified. j) The
9、 text of subclause 10.1 “Method of calculation” has been deleted and subclause 10.1.1 “General” has been included. k) The former subclause 10.1.1 “Determination on product as received” has been divided into two subclauses (new 10.1.2 and 10.1.3) “except” and “for sunflower seed”. l) Subclauses 11.2
10、and 11.3 have been modified with regard to the “absolute difference” between two test results (reference is made to Annex A). m) The results of interlaboratory tests have been updated on the basis of new interlaboratory tests. n) The bibliography has been updated. o) The standard has been brought in
11、 line with the current rules of presentation. DIN EN ISO 659:2009-11 3 Previous editions DIN EN ISO 659: 1998-10 National Annex NA (informative) Bibliography DIN EN ISO 542, Oilseeds Sampling DIN EN ISO 658, Oilseeds Determination of content of impurities DIN EN ISO 664, Oilseeds Reduction of labora
12、tory sample to test sample DIN EN ISO 665, Oilseeds Determination of moisture and volatile matter content DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement m
13、ethods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN EN ISO 659:2009-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 659 July 2009 ICS 67.200.20 Supersedes EN ISO 659:199
14、8 English Version Oilseeds - Determination of oil content (Reference method) (ISO 659:2009) Graines olagineuses - Dtermination de la teneur en huile (Mthode de rfrence) (ISO 659:2009) lsamen - Bestimmung des lgehaltes (Referenzverfahren) (ISO 659:2009) This European Standard was approved by CEN on 3
15、 June 2009. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be o
16、btained on application to the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Man
17、agement Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, No
18、rway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any for
19、m and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 659:2009: EContents 2 DIN EN ISO 659:2009-11 EN ISO 659:2009 (E) Page Foreword .3 1 Scope4 2 Normative references4 3 Terms and definitions .4 4 Principle .4 5 Reagent.5 6 Apparatus.5 7 Sampling 6 8 Preparation of test sa
20、mple .6 8.1 Reduction of laboratory sample 6 8.2 Predrying6 8.3 Test sample7 9 Procedure.8 9.1 General .8 9.2 Test portion8 9.3 Determination 9 9.4 “Oil content” of impurities10 10 Expression of results10 10.1 Method of calculation10 11 Precision 13 11.1 Interlaboratory test programme.13 11.2 Repeat
21、ability 13 11.3 Reproducibility 13 12 Test report13 Annex A (informative) Results of interlaboratory tests on the determination of oil content14 Bibliography15 Foreword 3 collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their This European Standard
22、shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2010, and conflicting national standards shall be withdrawn at the latest by January 2010. Attention is drawn to the possibility that some of the elements of this
23、document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 659:1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries a
24、re bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Swe
25、den, Switzerland and the United Kingdom. Endorsement notice The text of ISO 659:2009 has been approved by CEN as a EN ISO 659:2009 without any modification. This document (EN ISO 659:2009) has been prepared by Technical Committee ISO/TC 34 “Food products” in by-products Methods of sampling and analy
26、sis” the secretariat of which is held by AFNOR. EN ISO 659:2009 (E) DIN EN ISO 659:2009-11 1 Scope This International Standard specifies a reference method for the determination of the hexane extract (or light petroleum extract), called the “oil content”, of oilseeds used as industrial raw materials
27、. The procedure for sunflower seed is different from those for other seeds as it includes an additional moisture content determination after the seed has been ground to prepare the test sample. The method has been tested on rapeseed, soya beans and sunflower seed. This does not, however, preclude it
28、s applicability to other commercial seeds. If required, the pure seeds and the impurities (see 9.4) can be analysed separately. In the case of groundnuts (see 10.1.6), the pure seeds, the total fines, the non-oleaginous impurities and the oleaginous impurities can be analysed separately. 2 Normative
29、 references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 658, Oilseeds Determination of co
30、ntent of impurities ISO 664, Oilseeds Reduction of laboratory sample to test sample ISO 665, Oilseeds Determination of moisture and volatile matter content 3 Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 hexane extract “oil cont
31、ent” all the substances extracted under the operating conditions specified in this International Standard, expressed as a percentage by mass of the product as received, or on the cleaned seed NOTE On request, it may be expressed relative to the dry matter. 4 Principle The oil is extracted from a tes
32、t portion, in a suitable apparatus, with hexane or light petroleum. The solvent is removed from the extract and the extract weighed. Due to the varied nature of seeds, there are some variations in the procedure for different seeds. 4 DIN EN ISO 659:2009-11 EN ISO 659:2009 (E) 5 Reagent 5.1 Technical
33、 hexane, n-hexane or light petroleum, essentially composed of hydrocarbons with six carbon atoms, of which less than 5 % distils below 40 C and more than 95 % distils between 40 C and 60 C or between 50 C and 70 C, and which has a bromine value of less than 1. The residue on complete evaporation sha
34、ll not exceed 2 mg per 100 ml. 6 Apparatus Usual laboratory apparatus and, in particular, the following: 6.1 Analytical balance, with an accuracy of 0,001 g. 6.2 Mechanical mill, easy to clean, appropriate for the nature of the oilseeds and allowing the oilseeds to be ground to a uniform particle si
35、ze without appreciable heating or change in moisture, volatile-matter or oil content. NOTE The following mills have been found to give satisfactory results: the Christy see 8.3.2, 8.3.3 and 8.3.4); the Retsch ZM 200 ultra-centrifugal mill2), with a 1 mm screen for sunflower seed or with other screen
36、s depending on seed type. Other mills may be satisfactory, provided they conform to the criteria given above. 6.3 Mechanical microgrinder, capable of producing a fineness of grind of the oilseeds of less than 160 m, with the exception of the “shell”, particles of which may reach 400 m. Coffee grinde
37、rs and similar cutting-action mechanical grinders shall not be used as microgrinders. NOTE A ball mill comprising a stainless-steel tube of volume approximately 120 ml and 1 cm, 2 cm and 3 cm diameter steel balls (weighing approximately 7 g, 30 g and 130 g), depending on the sample being ground, and
38、 utilizing extremely rapid shaking, has been found to be suitable. If the microgrinder and its closure are designed for use with solvents, a small amount (approximately 20 ml) of solvent may be added to the cylinder in order to increase the speed of the extraction. 6.4 Extraction thimble (cellulose)
39、 and cotton wool, free from matter soluble in hexane or light petroleum. 6.5 Suitable extraction apparatus, fitted with a flask of capacity 200 ml to 250 ml. Straight-through extractors, for example the Butt, Smalley or Bolton-Williams type, are preferred for safety reasons and have been found to gi
40、ve a more efficient extraction. The use of other extractors is conditional upon the results of a test on a standard material of known oil content to confirm the suitability of the apparatus. If a Soxhlet syphoning-type extractor is used then, for safety reasons, a 250 ml flask should be utilized and
41、 the volume of solvent used shall be at least 150 ml. This should prevent rapid boiling on syphoning, which could otherwise cause loss of solvent and/or part of the test portion. 6.6 Pumice stone, in small particles, or other anti-bumping granules, previously dried in an oven at (130 2) C and cooled
42、 in a desiccator. 2) The Christy for shell and dirt: grind for 10 min in a microgrinder (6.3) using a 3 cm steel ball. 8.3.3 Copra (and coconut) Freeze the entire sample before milling in the mechanical mill (6.2). A mechanical mill with a 6 mm screen has been found to be satisfactory. The length of
43、 the particles shall be approximately 2 mm but shall not be greater than 5 mm. Mix the particles carefully and carry out the determination without delay. Care shall be taken to avoid condensation of moisture onto the seeds during and after grinding. 8.3.4 Large- and medium-sized seeds (illipe nuts,
44、shea nuts, groundnuts, soya, etc., but NOT sunflower seed or cottonseed) Grind the test sample in the mechanical mill (6.2) until the major dimension of the particles obtained is not greater than 2 mm. Reject the first particles (about one-twentieth of the sample), collect the rest, mix carefully an
45、d carry out the determination without delay. The following milling techniques have been found to be satisfactory: for soya: a mechanical mill with a 0,8 mm perforated plate or with a 1 mm screen; for groundnuts: a mechanical mill with a 3 mm bar screen (with samples containing a mass fraction of mor
46、e than about 45 % of oil, care shall be taken to avoid, as far as possible, the formation of a pasty mass); other seeds: a mechanical mill with a 6 mm bar screen. 7 EN ISO 659:2009 (E) DIN EN ISO 659:2009-11 The grinding of very oily seeds can often be improved if the seeds are first frozen at 10 C
47、to 20 C, but great care shall be taken to avoid condensation of moisture onto the seeds during and after grinding. 8.3.5 Sunflower seed Determine the moisture and volatile-matter content of the sunflower seed (as received) on the whole seed in accordance with ISO 665, taking care to observe strictly
48、 the drying periods laid down in the method specified in ISO 665. Record the result of this moisture and volatile-matter determination (U1). Grind the test sample in a mechanical mill (6.2). During grinding, the mill shall be fed slowly with the sunflower seeds to prevent a paste being formed. A mec
49、hanical mill with a 1 mm screen has been found to be suitable. If a screen-type mill is not used, sieve through a 2 mm sieve and regrind the material which does not pass through the sieve until the major dimension of the particles is not greater than 2 mm. Collect all the sievings, mix carefully and, without delay, determine the moisture and volatile-matter content in accordance with ISO 665, taking care to observe strictly the drying periods laid down in ISO 665. Record the result of the moisture and volatil
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